Department of chemistry, Yasouj University, Yasouj, Iran.
J Sep Sci. 2013 Jun;36(11):1734-42. doi: 10.1002/jssc.201300085. Epub 2013 Apr 27.
A simple, rapid, and sensitive method based on dispersive liquid-liquid microextraction combined with HPLC-UV detection applied for the quantification of chlordiazepoxide in some real samples. The effect of different extraction conditions on the extraction efficiency of the chlordiazepoxide drug was investigated and optimized using central composite design as a conventional efficient tool. Optimum extraction condition values of variables were set as 210 μL chloroform, 1.8 mL methanol, 1.0 min extraction time, 5.0 min centrifugation at 5000 rpm min(-1), neutral pH, 7.0% w/v NaCl. The separation was reached in less than 8.0 min using a C18 column using isocratic binary mobile phase (acetonitrile/water (60:40, v/v)) with flow rate of 1.0 mL min(-1) The linear response (r(2) > 0.998) was achieved in the range of 0.005-10 μg mL(-1) with detection limit 0.0005 μg mL(-1) The applicability of this method for simultaneous extraction and determination of chlordiazepoxide in four different matrices (water, urine, plasma, and chlordiazepoxide tablet) were investigated using standard addition method. Average recoveries at two spiking levels were over the range of 91.3-102.5% with RSD < 5.0% (n = 3). The obtained results show that dispersive liquid-liquid microextraction combined with HPLC-UV is a fast and simple method for the determination of chlordiazepoxide in real samples.
一种基于分散液液微萃取结合高效液相色谱-紫外检测的简单、快速、灵敏的方法，用于某些实际样品中氯氮卓的定量分析。采用中心复合设计作为常规有效工具，考察并优化了不同萃取条件对氯氮卓药物萃取效率的影响。将变量的最佳萃取条件值设定为 210μL 氯仿、1.8mL 甲醇、1.0min 萃取时间、5000rpm min(-1)下 5.0min 离心、中性 pH 值、7.0%w/vNaCl。采用 C18 柱，在 8.0min 内可实现分离，采用等度二元流动相（乙腈/水（60:40，v/v）），流速为 1.0mL min(-1)。在 0.005-10μgmL(-1)范围内获得线性响应（r(2)>0.998），检测限为 0.0005μgmL(-1)。采用标准加入法考察了该方法在水、尿、血浆和氯氮卓片剂四种不同基质中同时萃取和测定氯氮卓的适用性。在两个加标水平的平均回收率在 91.3-102.5%范围内，RSD<5.0%（n=3）。结果表明，分散液液微萃取结合高效液相色谱-紫外检测法是一种快速、简单的测定实际样品中氯氮卓的方法。
